CN105887039A - Method for directly generating multiporous carbon nanofibers on nanoporous copper - Google Patents
Method for directly generating multiporous carbon nanofibers on nanoporous copper Download PDFInfo
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- CN105887039A CN105887039A CN201610377080.1A CN201610377080A CN105887039A CN 105887039 A CN105887039 A CN 105887039A CN 201610377080 A CN201610377080 A CN 201610377080A CN 105887039 A CN105887039 A CN 105887039A
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- temperature
- quartz boat
- copper
- carbon nanofibers
- reaction tube
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
- C23C16/26—Deposition of carbon only
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/02—Pretreatment of the material to be coated
- C23C16/0227—Pretreatment of the material to be coated by cleaning or etching
Abstract
The invention provides a method for directly generating multiporous carbon nanofibers on nanoporous copper. The method comprises the following steps: 1) preparing nanoporous copper; 2) preparing the multiporous carbon nanofibers, namely, feeding the nanoporous copper prepared in step 1 into a quartz boat; positioning the quartz boat into an external area of a reaction tubular hearth; charging acetylene, argon and hydrogen based on the flow ratio of 50: 500: 200; heating a furnace to be 700 to 1000 DEG C; quickly moving the quartz boat into a constant-temperature area in the middle of a reaction tube after the furnace is heated to reach the set temperature; roasting for 5 to 10 minutes under such temperature; opening a furnace cover after roasting; cooling a sample under argon atmosphere until the room temperature is reached, so as to obtain the multiporous carbon nanofibers generated on the nanoporous copper. The method is simple in preparation process, low in cost, and high in controllability; the obtained multiporous carbon nanofibers are high in purity and high in yield; the method is applicable to industrial production.
Description
Technical field
The present invention relates to a kind of method of direct growth porous carbon nanofiber on nano porous copper, belong to the preparing technical field of nano material.
Background technology
Porous carbon nanofiber is a kind of new carbon, has the most excellent process based prediction model, such as specific surface area big, mechanical strength
Height, electric conductivity, heat conductivity are good, thus are paid close attention to by every field, and especially in electrochemical field, abundant pore structure makes porous carbon receive
Rice fiber can be applied to high performance electrode material, such as electrochemical capacitance, lithium-sulfur cell, sodium electricity and fuel cell etc..
At present, electrostatic spinning technique is to prepare the method that porous carbon nanofiber is the most commonly used.But, electrostatic spinning technique is relatively costly, process
Complex, yield is relatively low, is not suitable for being prepared on a large scale porous carbon nanofiber.Again because of non-metal catalyst effect, the porous carbon finally given
The crystallization of nanofiber is the most on the low side, thus limits its application in electrochemical field.So high-volume, high-purity, high-crystallinity porous carbon are received
The preparation of rice fiber remains a problem demanding prompt solution.
Summary of the invention
For the deficiencies in the prior art, the technical problem that the present invention intends to solve is to provide a kind of direct growth porous carbon nanometer on nano porous copper
The method of fiber；The method process is simple, with low cost, controllability is good, and the porous carbon nanofiber purity obtained is high, yield is big, is suitable for work
Industry metaplasia is produced.The present invention solves the technical scheme of above-mentioned technical problem:
A kind of method of direct growth porous carbon nanofiber on nano porous copper, comprises the following steps:
1) nano porous copper is prepared
The proportion that atomic ratio is 3:7 to 4:6 selecting Cu and Mn chooses alloy foil sheet, and alloy foil sheet is placed in 0.04-0.06M's
In hydrochloric acid solution, utilize chemical method to carry out removal alloying and process 30-60 minute, prepare nanoporous copper foil, by prepared nano porous copper
Paillon foil is standby after cleaning；
2) porous carbon nanofiber is prepared
By step 1 prepare nano porous copper put in quartz boat, quartz boat is placed in reaction tube burner hearth perimeter, be passed through acetylene, argon and
Hydrogen, wherein, acetylene, argon, hydrogen ratio press the flow configuration of 50:500:200, now furnace temperature are risen to 700-1000 DEG C；Treat furnace temperature liter
To assigned temperature, quartz boat is quickly moved to flat-temperature zone in the middle part of reaction tube, at this temperature calcining 5-10 minute；By quartz boat after calcining
Quickly in the middle part of reaction tube, flat-temperature zone moves to outside burner hearth, and is opened by bell, under the atmosphere of argon, sample is down to room temperature, i.e. can get
The porous carbon nanofiber that nano porous copper grows above.
Compared with prior art, the inventive method has the advantage that (1) utilizes nano porous copper for template and catalyst, uses chemical gaseous phase
Sedimentation one step catalyzes and synthesizes porous carbon nanofiber, simplifies technological process, is greatly saved cost；(2) the porous carbon Nanowire prepared by
Dimension purity is high, and yield is big, and controllability is good, and preparation process and equipment simple, it is easy to accomplish industrial application.
Accompanying drawing explanation
Fig. 1 is that the present invention prepares nano porous copper SEM image；
Fig. 2 is the porous carbon nanofiber SEM image prepared by the present invention；
Fig. 3 is the porous carbon nanofiber TEM image prepared by the present invention；
Fig. 4 is the porous carbon nanofiber HRTEM image prepared by the present invention.
The present invention does not addresses part and is applicable to prior art.
Detailed description of the invention
The specific embodiment of preparation method of the present invention given below.These embodiments are only used for describing preparation method of the present invention in detail, are not limiting as this
Application scope of the claims.
Embodiment 1
Selecting thickness is the Cu of 100um40Mn60Alloy foil sheet, and it is cut into 1*1cm2Size.Then configuration concentration is the salt of 0.05M
Acid solution, immerses alloy foil sheet in hydrochloric acid solution, at room temperature carries out removal alloying.The removal alloying time is 40 minutes, and removal alloying is tied
After bundle, paillon foil is sequentially passed through deionized water-alcohol washes, puts into after cleaning up in vacuum drying oven, at room temperature vacuum drying 12 hours,
Obtain nano porous copper.Put into being dried nano porous copper completely in quartz Noah's ark, and Noah's ark is placed in reaction tube burner hearth perimeter, be passed through
Acetylene, argon and hydrogen, the ratio of three kinds of gases is C2H2:Ar:H2=50:500:200sccm.Meanwhile, tube furnace temperature is risen to 700 DEG C,
When furnace temperature arrives 700 DEG C, quartz Noah's ark is quickly moved to outside burner hearth flat-temperature zone in the middle part of reaction tube, at this temperature reaction 5 minutes.Reaction
After end, by quartz boat, quickly in the middle part of reaction tube, flat-temperature zone moves to outside burner hearth, and is opened by bell, closes acetylene and hydrogen, at argon
Under atmosphere, sample is down to room temperature, the porous carbon nanofiber of homoepitaxial can be obtained.
Embodiment 2
Selecting thickness is the Cu of 50um40Mn60Alloy foil sheet, and it is cut into 1*1cm2Size.Then configuration concentration is the salt of 0.05M
Acid solution, immerses alloy foil sheet in hydrochloric acid solution, at room temperature carries out removal alloying, and the removal alloying time is 20 minutes, and removal alloying is tied
After bundle, paillon foil is sequentially passed through deionized water-alcohol washes, puts into after cleaning up in vacuum drying oven, at room temperature vacuum drying 12 hours,
Obtain nano porous copper.Put into being dried nano porous copper completely in quartz Noah's ark, and Noah's ark is placed in reaction tube burner hearth perimeter, be passed through
Acetylene, argon and hydrogen, the ratio of three kinds of gases is C2H2:Ar:H2=50:500:200sccm.Meanwhile, tube furnace temperature is risen to 700 DEG C,
When furnace temperature arrives 700 DEG C, quartz Noah's ark is quickly moved to outside burner hearth flat-temperature zone in the middle part of reaction tube, at this temperature reaction 10 minutes.Reaction
After end, by quartz boat, quickly in the middle part of reaction tube, flat-temperature zone moves to outside burner hearth, and is opened by bell, closes acetylene and hydrogen, at argon
Under atmosphere, sample is down to room temperature, the porous carbon nanofiber of homoepitaxial can be obtained.
Embodiment 3
Selecting thickness is the Cu of 200um40Mn60Alloy foil sheet, and it is cut into 1*1cm2Size.Then configuration concentration is the salt of 0.05M
Acid solution, immerses alloy foil sheet in hydrochloric acid solution, at room temperature carries out removal alloying, and the removal alloying time is 60 minutes, and removal alloying is tied
After bundle, paillon foil is sequentially passed through deionized water-alcohol washes, puts into after cleaning up in vacuum drying oven, at room temperature vacuum drying 12 hours,
Obtain nano porous copper.Put into being dried nano porous copper completely in quartz Noah's ark, and Noah's ark is placed in reaction tube burner hearth perimeter, be passed through
Acetylene, argon and hydrogen, the ratio of three kinds of gases is C2H2:Ar:H2=50:500:200sccm.Meanwhile, tube furnace temperature is risen to 900 DEG C,
When furnace temperature arrives 900 DEG C, quartz Noah's ark is quickly moved to outside burner hearth flat-temperature zone in the middle part of reaction tube, at this temperature reaction 10 minutes.Reaction
After end, by quartz boat, quickly in the middle part of reaction tube, flat-temperature zone moves to outside burner hearth, and is opened by bell, closes acetylene and hydrogen, at argon
Under atmosphere, sample is down to room temperature, the porous carbon nanofiber of homoepitaxial can be obtained.
Embodiment 4
Selecting thickness is the Cu of 100um40Mn60Alloy foil sheet, and it is cut into 1*1cm2Size.Then configuration concentration is the salt of 0.05M
Acid solution, immerses alloy foil sheet in hydrochloric acid solution, at room temperature carries out removal alloying, and the removal alloying time is 40 minutes, and removal alloying is tied
After bundle, paillon foil is sequentially passed through deionized water-alcohol washes, puts into after cleaning up in vacuum drying oven, at room temperature vacuum drying 12 hours,
Obtain nano porous copper.Put into being dried nano porous copper completely in quartz Noah's ark, and Noah's ark is placed in reaction tube burner hearth perimeter, be passed through
Acetylene, argon and hydrogen, the ratio of three kinds of gases is C2H2:Ar:H2=50:500:200sccm.Meanwhile, tube furnace temperature is risen to 800 DEG C,
When furnace temperature arrives 800 DEG C, quartz Noah's ark is quickly moved to outside burner hearth flat-temperature zone in the middle part of reaction tube, at this temperature reaction 10 minutes.Reaction
After end, by quartz boat, quickly in the middle part of reaction tube, flat-temperature zone moves to outside burner hearth, and is opened by bell, closes acetylene and hydrogen, at argon
Under atmosphere, sample is down to room temperature, the porous carbon nanofiber of homoepitaxial can be obtained.
Claims (1)
1. a method for direct growth porous carbon nanofiber on nano porous copper, comprises the following steps:
1) nano porous copper is prepared
The proportion that atomic ratio is 3:7 to 4:6 selecting Cu and Mn chooses alloy foil sheet, and alloy foil sheet is placed in 0.04-0.06M's
In hydrochloric acid solution, utilize chemical method to carry out removal alloying and process 30-60 minute, prepare nanoporous copper foil, by prepared nano porous copper
Paillon foil is standby after cleaning；
2) porous carbon nanofiber is prepared
By step 1 prepare nano porous copper put in quartz boat, quartz boat is placed in reaction tube burner hearth perimeter, be passed through acetylene, argon and
Hydrogen, wherein, acetylene, argon, hydrogen ratio press the flow configuration of 50:500:200, now furnace temperature are risen to 700-1000 DEG C；Treat furnace temperature liter
To assigned temperature, quartz boat is quickly moved to flat-temperature zone in the middle part of reaction tube, at this temperature calcining 5-10 minute；By quartz boat after calcining
Quickly in the middle part of reaction tube, flat-temperature zone moves to outside burner hearth, and is opened by bell, under the atmosphere of argon, sample is down to room temperature, i.e. can get
The porous carbon nanofiber that nano porous copper grows above.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610377080.1A CN105887039A (en) | 2016-05-30 | 2016-05-30 | Method for directly generating multiporous carbon nanofibers on nanoporous copper |
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| CN201610377080.1A CN105887039A (en) | 2016-05-30 | 2016-05-30 | Method for directly generating multiporous carbon nanofibers on nanoporous copper |
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| CN105887039A true CN105887039A (en) | 2016-08-24 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107739869A (en) * | 2017-11-09 | 2018-02-27 | 天津工业大学 | Nanoporous carbon/carbon-copper composite material and preparation method thereof |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102351164A (en) * | 2011-06-22 | 2012-02-15 | 天津大学 | Method for directly growing vertical nano carbon fiber arrays on copper matrix |
| CN103508438A (en) * | 2013-09-29 | 2014-01-15 | 天津大学 | Method for directly growing bamboo-like carbon nanometer tube on nano-porous copper |
| CN103738935A (en) * | 2013-12-13 | 2014-04-23 | 天津大学 | Method for preparing porous carbon material by using porous copper as template |
| CN105217617A (en) * | 2015-10-22 | 2016-01-06 | 天津大学 | A kind of preparation method of three-D nano-porous Graphene |
-
2016
- 2016-05-30 CN CN201610377080.1A patent/CN105887039A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102351164A (en) * | 2011-06-22 | 2012-02-15 | 天津大学 | Method for directly growing vertical nano carbon fiber arrays on copper matrix |
| CN103508438A (en) * | 2013-09-29 | 2014-01-15 | 天津大学 | Method for directly growing bamboo-like carbon nanometer tube on nano-porous copper |
| CN103738935A (en) * | 2013-12-13 | 2014-04-23 | 天津大学 | Method for preparing porous carbon material by using porous copper as template |
| CN105217617A (en) * | 2015-10-22 | 2016-01-06 | 天津大学 | A kind of preparation method of three-D nano-porous Graphene |
Non-Patent Citations (1)
| Title |
|---|
| JIANLI KANG ET AL: "Direct synthesis of fullerene-intercalated porous carbon nanofibers by chemical vapor deposition", 《CARBON》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107739869A (en) * | 2017-11-09 | 2018-02-27 | 天津工业大学 | Nanoporous carbon/carbon-copper composite material and preparation method thereof |
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Application publication date: 20160824 |
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